CAJ | 학술논문

建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5~100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％~98.9％，相对标准偏差为3.85％~4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。
건립료분석측정수배경중십록동적액상색보-천련질보법。수양경액액췌취、정화후，채용 Eclipse plus C18주（100 mm×2.1 mm，3.5μm）분리，을정화수위류동상진행제도세탈，재전분무부리자다반응감측모식하진행검측，동위소내표법정량。결과표명：채용액상색보-질보련용기술，증실료십록동재갑순중이반축철적형식존재，이재병동/을정중이해이순적형식존재。유우십록동겁성교강，재정화시난이세탈，병차불내산，소이불능여기타유궤록농약일기분석。십록동재5~100μg / L 범위유량호적선성관계，상관계수 r2=0.999，검출한급정량한분별위0.70 ng / L 화2.8 ng / L；재5、40화100 ng / L 3개농도첨가수평적평균회수솔위95.1％~98.9％，상대표준편차위3.85％~4.72％。본방법구유량호적령민도、회수솔화중현성，괄용우수배경중십록동적측정。
An analytical procedure for the determination of kepone in water was described. Water samples were extracted by liquid-liquid extraction,and then cleaned-up. Chromatograph-ic separation was performed on an Eclipse plus C18 column(100 mm×2. 1 mm,3. 5 μm)with gradient elution using acetonitrile and water at a flow rate of 0. 3 mL / min. The target com-pounds were determined in multiple reaction monitoring(MRM)mode via negative electrospray ionization( ESI - )and quantified by isotopic-dilution technique. Results showed that kepone existed as diol form and hemiacetal in acetone / acetonitrile and methanol respectively,the structures of which were confirmed by liquid chromatography-tandem mass spectrometry( LC-MS / MS). Due to the polar nature of kepone,it was difficult to be eluted during clean-up proce-dure and it may be decomposed during sulfuric acid washing. Therefore,it could not be ana-lyzed together with the other organochlorine pesticides. The calibration curve showed good line-arity in the range of 5-100 μg / L with correlation coefficient(r 2 )of 0. 999. The limit of detec-tion was 0. 70 ng / L and the limit of quantification was 2. 8 ng / L in water. The average recover-ies when spiked at 5,40 and 100 ng / L in water were 95. 1% -98. 9% ,and the relative standard deviations(RSDs)were 3. 85% -4. 72% . The method can be used to the determination of kepone in water due to its high sensitivity,good recovery and reproducibility.